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HJ 891-2017

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HJ 891-2017English459 ASK Days<=4 Solid waste. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method Valid HJ 891-2017
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Detail Information of HJ 891-2017; HJ891-2017
Description (Translated English): Solid waste. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z13
Classification of International Standard: 13.030.10
Word Count Estimation: 23,256
Date of Issue: 2017-12-17
Date of Implementation: 2018-02-01
Quoted Standard: HJ 77.3; HJ 782; HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300
Drafting Organization: Zhejiang Environmental Monitoring Center
Administrative Organization: Ministry of Environmental Protection
Regulation (derived from): Ministry of Environmental Protection Bulletin 2017 No. 73
Summary: This standard specifies gas chromatography-mass spectrometry for the determination of polychlorinated biphenyls in solid wastes and their leachate. This standard applies to the determination of 18 polychlorinated biphenyls in solid wastes and leachates. If verified, this standard also applies to the determination of other PCB congeners. When the solid waste sample volume is 20 g and the volume constant volume is 1.0 ml, the detection limit of 18 polychlorinated biphenyls is 2 to 3 ��g/kg, the lower limit of determination is 8 to 12 ��g/kg, and the solid waste leachate volume is 300 ml. When the constant volume was 1.0 ml, the method detection limit was 0.08-0.2 ��g/L and the lower limit of determination was 0.32-0.8 ��g/L. See Appendix A for details.

HJ 891-2017
(Solid waste - Determination of PCBs - Gas chromatography - mass spectrometry)
People's Republic of China national environmental protection standards
Solid waste - Determination of PCBs
Gas chromatography - mass spectrometry
Solid waste-Determination of polychlorinated biphenyls
-Gas chromatography mass spectrometry
2017-12-17 Published
2018-02-01 implementation
Ministry of Environmental Protection released
i directory
Foreword .ii
1 scope of application .1
2 Normative references .1
3 method principle .1
4 Reagents and materials .1
5 instruments and equipment .4
6 samples .4
7 Analysis steps .7
8 Results Calculation and Presentation 10
9 Precision and accuracy 11
10 Quality Assurance and Quality Control ..12
11 Waste treatment .12
Appendix A (Normative) Method detection limit and lower limit of determination
Appendix B (informative) Gel permeation chromatography calibration standard solution peak .14
Appendix C (Informative) Quantitative ions, auxiliary ions and their ion abundance ratio .15
Appendix D (informative) method of precision 16
Appendix E (Informative) Method Accuracy 19
Foreword
In order to carry out "Law of the People's Republic of China on Environmental Protection" and "Law of the People's Republic of China on Prevention and Control of Environmental Pollution by Solid Wastes"
Protect the environment, protect human health, standardize the determination of solid waste and leaching solution of PCBs, the development of this standard.
This standard specifies the determination of solid waste and leachate 18 kinds of PCBs by gas chromatography - mass spectrometry.
This standard Appendix A normative appendix, Appendix B ~ Appendix E is informative appendix.
This standard is released for the first time.
This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop.
This standard was drafted. Zhejiang Provincial Environmental Monitoring Center.
This standard verification unit. Jiangsu Provincial Environmental Monitoring Center, Hubei Provincial Environmental Monitoring Center, Hangzhou Environmental Monitoring Center,
Ningbo Environmental Monitoring Center, Shaoxing Environmental Monitoring Center Station and Jiaxing Environmental Monitoring Station.
This standard MEP approved on December 17,.2017.
This standard since February 1,.2018 implementation.
This standard is interpreted by the MEP.
Solid waste - Determination of PCBs - Gas chromatography - mass spectrometry
Warning. The standard substances and solvents used in the experiment are all toxic substances. The preparation process should be carried out in a fume hood.
And pay attention to wear protective equipment, avoid contact with skin and clothing.
1 scope of application
This standard specifies the determination of solid waste and its leachate PCBs by gas chromatography - mass spectrometry.
This standard applies to the determination of 18 kinds of PCBs in solid waste and leachate. If verified, this standard is also suitable
For other polychlorinated biphenyls congeners determination.
When the solid waste sample volume is 20 g and the constant volume is 1.0 ml, the detection limits of the 18 PCBs are 2 to 3
g/kg, the lower limit of determination is 8 ~ 12 g/kg; solid waste leachate volume of 300 ml, volume of 1.0 ml, the side
The detection limit was 0.08 ~ 0.2 g/L, and the lower limit of determination was 0.32 ~ 0.8 g/L. See Appendix A for details.
2 Normative references
This standard references the following documents or the terms. For undated references, the effective version applies to this book
standard.
HJ 77.3 Solid waste Dioxins Determination Isotope dilution High-resolution gas chromatography-high resolution mass spectrometry
HJ 782 Solid waste - Extraction of organic matter - Pressurized fluid extraction
HJ/T 20 Industrial solid waste sampling Sampling specifications
HJ/T 298 Hazardous Waste Identification Technical Specifications
Solid waste extraction toxicity Toxicity method HNO3 method
HJ/T 300 solid waste leaching toxic leaching method acetic acid buffer solution method
3 method principle
PCBs in solid wastes are extracted by Soxhlet or pressurized fluid extraction. PCBs in leachate
Using liquid-liquid extraction, the extraction liquid selected appropriate methods of purification, concentration and separation by gas chromatography - mass spectrometry, detection, according to
Retention time and characteristic ion abundance ratio qualitative, internal standard method.
4 Reagents and materials
Unless otherwise specified, the analysis of the use of analytical reagents in line with national standards, the experimental water for the newly prepared non-containing head
Standard water, subject to a blank test before use.
4.1 acetone (C3H6O). pesticide grade.
4.2 Toluene (C7H8). pesticide residues.
4.3 n-hexane (C6H14). pesticide grade.
4.4 methanol (CH3OH). pesticide grade.
24.5 Dichloromethane (CH 2 Cl 2). Pesticide grade.
4.6 Dimethyl sulfoxide (C2H6OS).
Saturated with n-hexane (4.3) before use.
4.7 Hydrochloric acid.  (HCl) = 1.18 g/ml, excellent grade pure.
4.8 Sulfuric acid.  (H2SO4) = 1.84 g/ml, excellent grade pure.
4.9 Sodium hydroxide (NaOH). excellent grade pure.
4.10 Potassium hydroxide (KOH). excellent pure grade.
4.11 Sodium chloride (NaCl).
Heat at 450 ° C for 4 h, cool to room temperature in a desiccator and store in a clean reagent bottle.
4.12 anhydrous sodium sulfate (Na2SO4). excellent grade pure.
660 ℃ calcined 6 h, cooled to 150 ℃ after the transfer to the dryer, after cooling into the reagent bottle, stored in a desiccator.
4.13 Dichloromethane - n-hexane mixed solvent. 3 7.
Dichloromethane (4.5) and n-hexane (4.3) were mixed at a volume ratio of 3.7.
4.14 n-hexane - acetone mixed solvent. 1 1.
Hexane (4.3) and acetone (4.1) were mixed in a volume ratio of 1.1.
4.15 hydrochloric acid solution. 1 1.
Hydrochloric acid (4.7) and water were mixed in a volume ratio of 1.1.
4.16 Sodium hydroxide solution.  (NaOH) = 40 mg/L.
Weigh 4 g of sodium hydroxide (4.9) and dilute to 100 ml with water.
4.17 Potassium hydroxide solution.  (KOH) = 112 mg/L.
Weigh 11.2 g of potassium hydroxide (4.10) and dilute to 100 ml with water.
4.18 Sodium chloride solution.  (NaCl) = 50 mg/L.
Weigh 5 g of sodium chloride (4.11) and dilute to 100 ml with water.
4.19 PCB stock standard solution.  = 100 mg/L.
Buy a certified standard solution (polychlorinated biphenyls standard solution or single component polychlorinated biphenyl standard solution), - below 20 ℃
Protect from light, or refer to the standard solution certificate for instructions.
4.20 Polychlorinated biphenyls standard solution.  = 10.0 mg/L (reference concentration).
Dilute PCB stock standard solution (4.19) with n-hexane (4.3) or methanol (4.4). The solution is below -20 ℃ avoidance
Light preservation, can be stored for two months.
4.21 Internal standard stock solution.  = 100 mg/L.
Buy a certified standard solution. Choosing tetrachloro-m-xylene (TCMX) as an internal standard can also use deca-biphenyl and deuterium
Substitute polychlorinated biphenyls or isotope standards as internal standard, below -20 ℃ dark preservation, or reference to the standard solution certificate that
Save it.
4.22 Internal standard solution.  = 10.0 mg/L (reference concentration).
The internal standard stock solution (4.21) is diluted with n-hexane (4.3) or methanol (4.4). The solution at -20 ℃ below light preservation,
Can be kept for two months.
4.23 Replacement standard stock solution.  = 500 mg/L.
Buy a certified standard solution. 2,2 ', 4,4', 5,5'-hexabromobiphenyl (PBB-153) was chosen as the standard stock solution of substitutes,
3 It is also possible to use deca-biphenyl, deuterium-substituted PCBs or isotope standards as a substitute for the standard, keep it in the dark at -20 ° C,
Or refer to the standard solution certificate instructions for preservation.
4.24 Alternatives Standard solution.  = 40.0 mg/L (reference concentration).
Dilute the replacement standard stock (4.23) with n-hexane (4.3) or methanol (4.4). The solution below -20 ℃ dark
Save, can be saved for two months.
4.25 decafluorotriphenylphosphine (DFTPP) stock solution.  = 1000 mg/L, the solvent is methanol.
Buy a certified standard solution, stored below 4 ℃ dark, or refer to the standard solution certificate to save the relevant instructions.
4.26 Dodecafluorotriphenylphosphine (DFTPP) Solution.  = 50.0 mg/L.
Dilutetriphenylphosphine (DFTPP) stock solution (4.25) was diluted with methanol (4.4). Use liquid below -20 ℃ to avoid light
Save.
4.27 gel permeation chromatography calibration standard stock solution. corn oil ( = 300 mg/ml), diethylhexyl phthalate (
Pentahydrate ( = 1.4 mg/ml), pyrene ( = 0.1 mg/ml), elemental sulfur ( = 0.5 mg/ml)
Methylene chloride.
Buy a certified standard solution, 4 ℃ below the dark preservation, or refer to the standard solution certificate instructions for preservation.
4.28 gel permeation chromatography calibration standard solution. corn oil ( = 30.0 mg/ml), diethylhexyl phthalate (
= 1.5 mg/ml), pentachlorophenol ( = 0.14 mg/ml), pyrene ( = 0.01 mg/ml) and elemental sulfur ( = 0.05 mg/ml).
Dilute gel permeation chromatography calibration stock (4.27) with dichloromethane (4.5). 4 ℃ below dark preservation, can be guaranteed
Save six months.
4.29 Copper beads (powder). 1.5 mm in diameter (250 μm, 60 mesh).
Before using hydrochloric acid solution (4.15), toluene (4.2) were rinsed, placed in a desiccator to save.
4.30 Silicone. 75 ~ 150 μm (200 ~ 100 mesh).
Wash with dichloromethane (4.5) until all the methylene chloride volatilized, spread in the evaporating dish or beaker, the thickness is less than
10 mm, activated at 130 ℃ for 18 h and placed in a desiccator for 30 min. Into a closed container into the dryer
In save.
4.31 sodium hydroxide alkaline silica gel.
Take activated silica gel (4.30) 67 g, sodium hydroxide solution (4.16) 33 g, stir, make it a fluid powder
Last shape. After the preparation is completed, the glass bottle is sealed and stored in a desiccator.
4.32 Silica gel.
Take activated silica (4.30) 100 g, add 78.6 g sulfuric acid (4.8), stir, make it into a fluid powder.
After the preparation is completed, it is sealed in a reagent bottle and stored in a desiccator.
4.33 10% Silver Nitrate Silicone. Commercial, protected from light.
4.34 Magnesium silicate. 150 ~ 250 μm (100 ~ 60 mesh).
Activate at 130 ° C for 18 h before use. Placed in a desiccator cooled to room temperature, sealed and stored in a clean reagent bottle
in. Preparation before use.
4.35 Diatomaceous earth. 38 ~ 150 μm (400 ~ 100 mesh).
Baking at 450 ℃ for 4 h, placed in a desiccator cooled to room temperature, transferred to a ground glass jar, stored in a desiccator.
4.36 quartz sand. 297 ~ 840 μm (50 ~ 20 mesh).
Baking at 450 ℃ for 4 h, placed in a desiccator cooled to room temperature, transferred to a ground glass jar, stored in a desiccator.
44.37 glass wool.
Before use, with dichloromethane (4.5) reflux extraction 24 h, dried and stored in airtight glass containers.
4.38 high purity nitrogen. purity ≥ 99.999%.
4.39 high purity helium. purity ≥ 99.999%.
5 instruments and equipment
5.1 Gas Chromatography-Mass Spectrometer (GC-MS). Equipped with capillary split/splitless inlet, with constant flow or constant pressure
Can; oven temperature programmable; with electron bombardment source (EI source).
5.2 Column. Low loss quartz capillary column. Column I. 30 m (length) 0.25 mm (ID) × 0.25 μm (film
Thick), the stationary phase is 5% phenyl 95% methylpolysiloxane. Column II. 60 m (length) 0.25 mm (ID), fixed
Phase modified 5% phenyl 95% methylpolysiloxane. Other equivalent low-loss columns are also available.
NOTE. In order to ensure that the chlorine-substituted PCBs of interest are well separated, capillaries of different properties may be selected in case of interference
Column check.
5.3 freeze-drying equipment.
5.4 Extraction device
5.4.1 Soxhlet extractor or equipment with considerable functionality.
5.4.2 Pressurized fluid extractor. with about 40 ml extraction cell, the extraction pressure of more than 1 500 psi, the extraction temperature needs
Greater than 120 ° C.
5.5 Purification device
5.5.1 Column. Glass column with inner diameter of 8 ~ 15 mm and length of.200 ~ 300 mm.
5.5.2 Automatic Gel Permeation Chromatography. with UV detector (254 nm wavelength) and length 600 mm, diameter 25 mm
Gel column packed with about 70 g of porous polystyrene divinylbenzene bioactive microspheres filler, 5 ~ 10 ml sample quantitative
ring.
5.6 Concentration device. rotary evaporation concentrator, nitrogen blowing instrument or other functionally equivalent enrichment device.
5.7 Metal sieve. 840 μm (20 mesh).
5.8 General laboratory equipment and equipment.
6 samples
6.1 Sample Collection and Storage
Solid waste samples were collected and prepared according to HJ/T 20 and HJ/T 298 requirements. After sample collection
4 ℃ under dark storage, 14 days to complete the extraction, within 40 d to complete the analysis of the extract.
6.2 Sample Preparation
6.2.1 Solid waste
Weigh 20.0 g sample, add an appropriate amount of anhydrous sodium sulfate (4.12), the sample was dried and mixed sand-like flow, spare.
If using pressurized fluid extraction, dehydrate with diatomaceous earth (4.35). Or directly selected after grinding sieved sample extraction.
5 Note 1. For large particles or hard solid waste samples that can not be agitated and can only be treated by crushing or other suitable air-dried or
Lyophilized samples may be dewatered using freeze-drying equipment (5.3) or other means and ground through a metal sieve (5.7), but should be considered
To low chlorinated PCBs loss.
Note 2. Sampling capacity can be adjusted according to sample type, degree of interference, pollutant content and extraction method. For organic pollutants with high content
Of the sample, may be appropriate to reduce the sample size, or take part of the extract for purification analysis.
6.2.2 solid waste leachate
Prepare solid waste leachate according to HJ/T 299 or HJ/T 300.
6.3 Sample Preparation
6.3.1 Extraction
6.3.1.1 Solid waste
6.3.1.1.1 Water-soluble and oily liquid solid waste
Weigh 20.0 g sample, add 80 ml of water and 50  l replacement of the standard solution (4.24), after mixing all transferred to the points
Liquid funnel, extracted with 100 ml of dichloromethane (4.5) three times, and the extract was dehydrated with anhydrous sodium sulfate (4.12)
Collected in a concentrate bottle.
Note. If the extract contains a lot of oil, you can refer to HJ 77.3 using dimethyl sulfoxide extraction method to remove hydrocarbons such as low polarity
After organic matter, and then 6.3.3 purification. Specific measures are as follows. The extract solvent was converted to n-hexane, concentrated to 3 ml left
Right, added to 25 ml of dimethylsulfoxide saturated with n-hexane (4.6), and the concentrate was washed three times with n-hexane (4.3)
Transferred to a solution of dimethyl sulfoxide, with a separatory funnel shaking extraction four times to collect about 100 ml of dimethylsulfoxide solution; collected
100 ml dimethyl sulfoxide solution was added 40 ml of n-hexane (4.3) shaken extraction, n-hexane was discarded; further dimethyl sulfoxide solution
75 ml of n-hexane (4.3) and 100 ml of water were added and the mixture was extracted by shaking. After standing, the n-hexane layer was collected and the operation was repeated three times.
And n-hexane was collected; to a hexane solution was added potassium hydroxide solution (4.17) 10 ml, shaking wash, discard the water layer and then
After adding 25 ml of water to wash and standing, the n-hexane extracts were dehydrated in anhydrous sodium sulfate (4.12) and collected in a concentrating flask.
6.3.1.1.2 Solid and semi-solid waste
a) Soxhlet extraction
Dehydrated sample (6.2.1) all transferred to the Soxhlet extractor (5.4.1) extraction cup, in each sample plus
Into 50  l replacement standard solution (4.24). With.200 ~ 300 ml n-hexane - acetone mixed solvent (4.14) or toluene
(4.2) solvent extraction more than 8 h, reflux rate control in 4 to 6 times/h, collecting the extract.
b) Pressurized fluid extraction
With reference to HJ 782 will dehydrated samples (6.2.1) all transferred to a suitable extraction tank, while adding 50 替 l instead
Standard standard solution (4.24). Set the extraction conditions, the pressure of 1 500 psi, a temperature of 120 ℃, the extraction solvent for n-hexane
- acetone mixed solvent (4.14) or toluene (4.2) solution, 100% full extraction cell mode, high temperature and pressure stand 5 min,
Loop three times and collect the extract.
Note. In the premise of meeting the quality control requirements of this method, other extraction solvents may be used after verification.
6.3.1.2 solid waste leachate
6 take solid waste leachate (6.2.2) 300 ml in a separatory funnel, add 40  l replacement standard solution (4.24),
Extract according to 6.3.1.1.1 Procedure and collect the extract.
6.3.2 extract (extract) concentration
The sample extract or extract (6.3.1) was transferred to the concentration device, concentrated to 1 ~ 2 ml, to be purified. Such as extraction
The solution is dichloromethane, concentrated to about 10 ml added 3 ml n-hexane (4.3) conversion solvent, continue to concentrate to 1 ~ 2 ml,
To be purified analysis.
6.3.3 Purification and separation
6.3.3.1 sulfur purification
Such as samples containing large amounts of sulfur, you need to first desulfurization purification.
In the concentrated extract (6.3.2) add about 50 ml of n-hexane (4.3), then add 15 g of copper beads after treatment
(Powder) (4.29), the full oscillation, filtration, the filtrate was concentrated to 1 ~ 2 ml, according to 6.3.3.3 method of purification.
6.3.3.2 sulfuric acid purification
If the extract color darker, you can use sulfuric acid purification method for the initial purification treatment.
The concentrated extract or extract (6.3.2) was transferred to a 125 ml separatory funnel, 75 ml of n-hexane
(4.3). Shake with 5-10 ml of sulfuric acid (4.8) for about 1 min. Discard the aqueous phase after standing and repeat until the sulfuric acid layer is clear
color. To the separatory funnel was added 30 ml of sodium chloride solution (4.18) to wash the organic phase, put it aside after stratification, the organic phase
Phase anhydrous sodium sulfate (4.12) after drying dehydration, concentrated to 1 ~ 2 ml, and then 6.3.3.3 or 6.3.3.4 purification method.
6.3.3.3 Multi-layer silica gel column purification
Add some glass wool (4.37) to the bottom of the glass column (inner diameter 12 ~ 15 mm) and add 3 g
Silica gel (4.30), 5 g basic sodium hydroxide (4.31), 2 g silica gel (4.30), 10 g silica gel (4.32), 2 g
Silica gel (4.30), 5 g of 10% silver nitrate silica gel (4.33, optional with minor sulfur interference) and 5 g of anhydrous sodium sulfate (4.12).
After filling, the multi-layer silica gel column was rinsed with 100 ml of n-hexane (4.3), keeping the liquid level in the anhydrous sodium sulfate layer.
Transfer concentrated extract or extract (6.3.2), or 6.3.3.1,6.3.3.2 purified concentrate to the purification column
Wash the wall of the extract with 1 to 2 ml of n-hexane (4.3) and repeat 2 to 3 times. Use 120 ml n-hexane
(4.3) at a flow rate of 2.5 ml/min (1 drop per second) to collect the eluate. Concentrate with concentrator to 1 ~ 2 ml, press
According to 6.3.3.4 steps further purification treatment, or directly concentrated to 1 ml or less, add 25 l internal standard solution (4.22)
Set the volume to 1.0 ml, to be measured.
6.3.3.4 Magnesium silicate column purification
When the sample is contaminated with organochlorine pesticides or other small molecules, it is necessary to purify 6.3.3.2 sulfuric acid or 6.3.3.3
The purified silica gel column samples were further purified using magnesium silicate chromatography.
Add some glass wool (4.37) to the bottom of the glass column (inner diameter 8 ~ 10 mm) and fill with 5 g
Anhydrous sodium sulfate (4.12), 5 g of magnesium silicate (4.34) and 5 g of anhydrous sodium sulfate (4.12) were treated with 40 ml of n-hexane (4.3)
Rinse the magnesium silicate column, keeping the liquid level in the anhydrous sodium sulfate layer. Purge 6.3.3.2 sulfuric acid or 6.3.3.3 multi-layer silica gel column
After the transfer of the concentrated liquid were all transferred to the column, with 1 ~ 2 ml of n-hexane (4.3) rinse the sample concentration flask three times, with the transfer
7 to the column, when the liquid level reaches the sodium sulfate layer, discard the eluent. Then add 100 ml of dichloromethane - n-hexane mixed solution
(4.13) eluting the column, the elution flow rate controlled at 2.5 ml/min (1 drop per second) or so, to receive the entire eluent.
Concentrate to 1 ml with a concentrator, add 25 l internal standard solution (4.22) volume to 1.0 ml, to be tested.
6.3.3.5 Automatic gel permeation chromatography (GPC) purification
When there is a macromolecular interference in the sample, you can choose automatic gel permeation chromatography of the concentrated extract or extract (6.3.2)
Purification, and then use 6.3.3.3 or 6.3.3.4 method to further purify the separation, you can also direct condensation volume analysis.
Dilute the eluent using methylene chloride (4.5) for automatic gel permeation chromatography. Inject 5 ml gel permeation color
Spectral calibration standards Use the solution (4.28) in the sample loop, using dichloromethane (4.5) to automatically elute the calibration standard,
Record UV detector response signal. The order of the normal chromatographic peaks is corn oil, diethylhexyl phthalate,
Chlorophenols, pyrene and sulfur, see Appendix B.
Set the PCB collection period. More than 85% of corn oil signal peak out, and more than 85% of phthalic acid two
Ethylhexyl ester can be collected at the point in time for the sample to begin collection, and the minimum signal peak time between the pyrene and sulfur signals is the sample
End collection time.
The concentrated extract or extract (6.3.2) with dichloromethane (4.5) volume to 10 ml, accurately remove 5 ml
The sample was eluted with dichloromethane (4.5) in a quantitative loop and the eluent was collected during the PCB time period. Concentrate and elute
Liquid to 10 ml added 3 ml of n-hexane (4.3), continue to concentrate to 1 ~ 2 ml, and then press 6.3.3.3 or 6.3.3.4 method further
Separation and purification, or continue to concentrate to 1 ml or less, add 25 l internal standard solution (4.22) volume to 1.0 ml, to be tested.
Note 1. Gel Permeation Chromatography calibration is required after every 20 samples to be processed in the automatic gel permeation chromatography
Recognition, such as pentachlorophenol recovery higher than 85%, then that the purification is effective, such as pentachlorophenol recovery of less than 85%, you need to front
1 batches of samples were extracted and purified.
Note 2. In the premise of meeting the quality control requirements of this method, other automatic or manual extraction and purification methods may be used after verification.
6.4 blank sample preparation
The actual sample was replaced with quartz sand (4.36), and solid waste was prepared separately according to the same procedure as sample preparation (6.3)
White samples and solid waste leachate Blank samples.
7 Analysis steps
7.1 Instrument reference conditions
7.1.1 Gas Chromatograph
Column I. program temperature mode, the starting temperature of 80 ℃ for 1 min, 10 ℃/min heating to 210 ℃, then 3 ℃/min
The temperature was raised to 226 ° C, and the temperature was raised to 305 ° C at 20 ° C/min for 20 min. Carrier gas. High-purity helium (4.39); Flow rate.
1.0 ml/min.
Column II. temperature program mode, the initial temperature of 130 ℃ for 1 min, 15 ℃/min heating to 210 ℃, and then
3 ℃/min heated to 310 ℃ for 20 min. Carrier gas. High-purity helium (4.39); Flow rate. 1.2 ml/min.
Injection mode. splitless injection, 0.75min after the start of diversion, diversion ratio 20.1. Injection volume. 1.0 μl. Inlet
Temperature. 280 ℃. Transmission line temperature. 280 ℃.
87.1.2 Mass Spectrometer
Ion source temperature. 250 ℃; Ion source electron energy. 70 eV; Quadrupole temperature. 150 ℃; Data acquisition mode.
Full scan mode (SCAN method) or select the ion method (SIM method). Solvent delay time. 4 min. Reference to the rest of the parameters
Set the instrument manual.
Quantitation and accessory ions of different numbers of chlorine-substituted PCBs (including internal standards and substitutes), and their ions
Abundance ratio see Appendix C.
7.2 Calibration
7.2.1 instrument performance check
Sample analysis before taking 1 十l decafluorotriphenylphosphine (DFTPP) liquid (4.26) direct injection of gas chromatography -
Mass spectrometry system instrument performance check, the abundance of the resulting mass ion should meet the requirements of Table 1.
Table 1 DFTPP key ions and ion abundance evaluation table
Mass ion m/z abundance evaluation Mass ion m/z abundance evaluation
51 Strength 30% ~ 60% of 198 fragments.199 Strength 5% ~ 9% of 198 fragments
68 2% strength less than 69 pieces 275 10% ~ 30% strength 198 pieces,
70 2% less than 69 sharpening 365 365% greater than 1%
127 Strength 40% to 60% of 198 fragments 441 Existence but not exceeding the strength of 443 fragments
197 1% of the intensity less than 198 fragments 442 40% of the intensity greater than 198 fragments
198 base peak, the relative intensity of 100% 443 intensity of 442 fragments of 17% to 23%
7.2.2 Preparation and determination of standard curve
Use PCB standard solution (4.20), alternative standard solution (4.24) and internal standard solution (4.22) to a
Alcohol (4.4) or n-hexane (4.3) as the solvent standard solution series, wherein the target compound concentration. 0.050 g/ml,
0.100 g/ml, 0.250 g/ml, 0.500 g/ml, 1.00 g/ml and 2.00 g/ml;
Degrees. 0.200 g/ml, 0.400 g/ml, 1.00 g/ml, 2.00 g/ml, 4.00 g/ml and 8.00 g/ml;
Liquid concentrations were 0.250  g/ml.
According to the instrument reference conditions (7.1) were analyzed to obtain different concentrations of the target compound mass spectrometry total ion current diagram,
The retention time of each target compound and the peak area of the ion mass spectrum peak were recorded. PCBs Reference material Total ion
Flow diagram shown in Figure 1.
7.2.3 Calculation of the average relative response factor
According to equation (1) and equation (2), the relative response factor and average relative response of standard series of target compounds were calculated
Factor, and calculate the relative standard deviation of the relative response factor.
Relative response factor (iRRF) according to equation (1) calculation.
i IS
IS i
RRF
 (1)
Where.
iRRF - relative response factor;
Ai - Quantum ion peak area of target compound in standard solution;
9IS - concentration of internal standard, g/ml;
AIS - peak area of internal standard quantitation ion;
i - concentration of target compound in standard solution, g/ml.
The average relative response factor (iRRF) according to equation (2) calculation.
RRF
RRF

(2)
Where.
iRRF - average relative response factor;
iRRF - relative response factor;
n - calibration series concentration point number.
1-TCMX (internal standard); 2-PCB-28; 3-PCB-52; 4-PCB-
PCB-156; PCB-157; PCB-156; PCB-157; PCB-
17-PCB-180; 18-PCB-169; 19-PCB-189; 20-PBB-153 (alternative).
Figure 1 PCBs total ion chromatogram (column I)
7.2.4 The establishment of standard curve
The ratio of the concentration of the target compound to the concentration of the internal standard is taken as the abscissa, and the target compound and the internal standard are used to quantify the ion peak area
The ratio of the vertical axis, using the least squares method to establish a standard curve. Non-linear fitting curves can also be used for calibration, but at least
There should be 6 concentration levels.
7.3 Determination
Take test sample (6.3) and test the sample in the same instrument conditions (7.2) as the standard curve. If try
Sample concentration of the test substance beyond the scope of the standard curve should be re-measured after dilution.
Note. When the sample is diluted, the internal standard should be properly added.
7.4 Blank test
Take a blank sample (6.4) and measure the blank sample according to the same instrument conditions as the sample test (7.3).
8 results calculated and said
8.1 Qualitative analysis
The retention time (RRT) of the target in the sample, the relative ion abundance ratio of the target ion and the target sample
Sex.
The relative retention time of the target compound in the sample to the desired retention time (ie, the average retention time in the standard sample)
Deviations should be controlled within ± 3%.
Samples of the target compound auxiliary qualitative ions and target ion abundance ratio should meet the requirements of Appendix C, the abundance ratio should be
Within ± 15% (concentration at the lower limit of determination should be within ± 25%).
Other chlorine-substituted polychlorinated biphenyls of the same type, which have been characterized, have different peak areas on the chromatogram that satisfy the requirements of Annex C
Seeking, and the distribution of different peaks showed a certain law, can be characterized as other PCBs congeners.
8.2 Quantitative analysis
According to the quantitative ion peak area, using internal standard method.
8.3 Calculation Results
8.3.1 Calculation results for PCBs in solid waste samples
The content of PCBs in solid waste samples, ωi, is calculated according to Eq. (3).
1i IS
iIS
AV
A mRRF
     (3)
Where.
ωi - the content of the target in the sample, μg/kg;
Ai - the peak area of the target ion in the sample;
AIS - peak area of internal standard compound ion in sample;
 IS - the concentration of the internal standard compound in the sample, g/ml;
iRRF - average relative response factor of target compound;
V1 - sample volume, ml;
m - sampling volume, kg;
D - dilution factor.
8.3.2 Calculations of PCBs in solid waste leachate samples
The concentration of PCBs in solid waste leachate, ρi, is calculated according to Eq. (4).
1i IS
IS i
AV
A VRRF
     (4)
Where.
i - the content of the target sample, μg/L;
Ai - peak area of the target compound in the sample to quantify ions;
AIS - peak area of internal standard compound ion in sample;
 IS - the concentration of the internal standard compound in the sample, g/ml;
iRRF - average relative response factor of target compound;
V1 - sample volume, ml;
V - sampling volume, L;
D - dilution factor.
8.4 results indicated
Solid waste was less than 100 μg/kg measured results, retained to the whole digit; determination of greater than or equal to 100 μg/kg,
Keep three significant figures.
Determination of solid waste leachate retained up to three significant figures, the effective digits after the decimal point retention and method detection
Limit the same.
9 precision and accuracy
9.1 Precision
Seven laboratories carried out spiked solid samples of PCBs containing 5.0 μg/kg and 25.0 μg/kg respectively
The repeatability was determined by the relative standard deviation in the laboratory ranged from 3.4% to 15% and from 2.7% to 16%
The standard deviations ranged from 10% to 22% and 3.2% to 18%, respectively, with reproducibility limits of 1 to 2 μg/kg and 1 to 8 μg/kg respectively
The current limit of 2 ~ 4 μg/kg and 2 ~ 14 μg/kg respectively. One laboratory spiked PCBs containing 100 μg/kg of solid waste
Samples were subjected to 6 replicate assays with relative standard deviations in the range of 3.6% to 11%.
Seven laboratories were 0.33 μg/L and 1.33 μg/L of fly ash solid waste leachate spiked samples for 6 times
Complex test, the relative standard deviation of the laboratory were 3.8% to 18% and 7.6% to 44%, relative standard laboratory
The standard deviation ranges from 12% to 29% and from 4.6% to 14%, respectively, with repeatability limits of 0.05 to 0.06 μg/L and 0.4 to 0.5
μg/L, reproducibility limits were 0.1 ~ 0.3 μg/L and 0.4 ~ 0.6 μg/L, respectively.
9.2 Accuracy
Seven laboratories separately measured the fly ash-based solid waste with the standard addition of 25.0 μg/kg for 6 times, and the recovery rate
The range of 82.5% ~ 137%, the final value of spiked recovery was 92.0% ± 9.8% ~ 103% ± 26%. A laboratory to the standard
The fly ash solid waste samples with the volume of 100 μg/kg were subjected to 6 replicate determinations and the recoveries ranged from 79.0% to 121%.
Seven laboratories separately measured the leachate of fly ash solid waste with the standard addition of 1.33 μg/L for 6 times,
The recoveries ranged from 56.1% to 88.8%. The final recoveries were 70.2% ± 15% -75.8% ± 21%.
For summary data of precision and accuracy, see Appendix D and Appendix E.
10 Quality Assurance and Quality Control
10.1 Blank test
At least one laboratory blank should be made for each batch of samples (no more than 20 samples) and the target compound concentration in the blank
It should be below the detection limit of the method.
10.2 Initial calibration
When using the average relative response factor of 7.2.3 for calibration, the relative standard deviation of relative response factors
The difference is less than 20%; the correlation coefficient of the standard curve established by 7.2.4 is ≥0.995. Otherwise, you should recalibrate.
10.3 Continuous calibration
Each time 20 samples are measured or at least one midpoint concentration of the calibration curve is measured every 24 h, the target compound
The relative error between the measured value and the standard value is within ± 20%.
10.4 Internal standard
Sample internal standard, continuous calibration of the internal standard and the curve of the midpoint of the internal standard comparison, the retention time does not exceed 10 s, the peak surface
The product change should be within -50% ~ 100%.
10.5 parallel sample determination
Each batch of samples (no more than 20 samples) should be at least one sample selected for parallel two-way test, solid sample level
The relative deviation of the determination result of the line is less than or equal to 25%, and the relative deviation of the parallel determination result of the solid waste leachate sample is less than or equal to 45%.
10.6 Substrate spiked sample determination
Each batch of samples (no more than 20 samples) should select at least one sample for matrix spiking test, solid sample plus
The standard recovery should be between 60% and 140%. The standard recovery of solid waste leachate should be between 50% and 120%.
10.7 Recovery of alternatives
The recovery rate of solid waste substitutes is between 65% and 140%. The recovery rate of solid waste leachate substitutes is between
45% ~ 120% between.
11 Waste treatment
The wastes generated by the laboratory shall be stored in categories and centrally stored, entrusted to qualified units for disposal.
Appendix A.
(Normative)
Method detection limit and determination of the lower limit
When the sampling volume of solid waste is 20.0 g, the sampling volume of solid waste leachate is 300 ml, and the solid waste is pressurized
Body extraction, extraction liquid using liquid-liquid extraction, the extract was purified with a multi-layer silica gel column, the volume was set at a constant volume of 1.0 ml,
Methods for detection and determination of 18 PCBs in solid waste and solid waste leachate are shown in Table A.1.
Table A.1 method detection limit and lower limit of determination
Compound Name Chemical Registration Number
IUPAC *
Numbering
Solid waste Solid waste leachate
The detection limit/
(Μg/kg)
Lower limit of determination /
(Μg/kg)
The detection limit/
(Μg/L)
Lower limit of determination /
(Μg/L)
1 2,4,4'-trichlorobiphenyl 7012-37-5 PCB-28 2 8 0.09 0.36
2 2,2 ', 5,5'-tetrachlorobiphenyl 35693-99-3 PCB-52 2 8 0.1 0.4
3 2,2 ', 4,5,5'-Pentachlorobenzene 37680-73-2 PCB-101 2 8 0.1 0.4
4 3,4,4 ', 5-tetrachlorobiphenyl 70362-50-4 PCB-81 2 8 0.1 0.4
5 3,3,4,4'-tetrachlorobiphenyl 32598-13-3 PCB-77 2 8 0.09 0.36
6 2 ', 3,4,4', 5-Pentachlorobenzene 65510-44-3 PCB-123 2 8 0.08 0.32
7 2,3 ', 4,4', 5-Pentachlorobenzene 31508-00-6 PCB-118 2 8 0.2 0.8
8 2,3,4,4 ', 5-Pentachlorobenzene 74472-37-0 PCB-114 2 8 0.1 0.4
9 2,2 ', 4,4', 5,5'-Hexachlorobiphenyl 35065-27-1 PCB-153 2 8 0.09 0.36
10 2,3,3 ', 4,4'-Pentachlorobenzene 32598-14-4 PCB-105 2 8 0.09 0.36
11 2,2 ', 3,4,4', 5'-HCB 35065-28-2 PCB-138 2 8 0.08 0.32
12 3,3 ', 4,4', 5-Pentachlorobenzene 57465-28-8 PCB-126 3 12 0.09 0.36
13 2,3 ', 4,4', 5,5'-hexachlorobiphenyl 52663-72-6 PCB-167 2 8 0.1 0.4
14 2,3 ', 4,4', 5-Hexachlorobiphenyl 38380-08-4 PCB-156 2 8 0.1 0.4
15 2,3,3 ', 4,4', 5'-Hexachlorobiphenyl 69782-90-7 PCB-157 2 8 0.09 0.36
16 2,2 ', 3,4,4', 5,5'-Heptachlorobiphenyl 35065-29-3 PCB-180 2 8 0.1 0.4
17 3,3 ', 4,4', 5,5'-Hexachlorobiphenyl 32774-16-6 PCB-169 2 8 0.2 0.8
18 2,3,3 ', 4,4', 5,5'-Heptachlorobiphenyl 39635-31-9 PCB-189 2 8 0.1 0.4
*. International Federation of Theoretical and Applied Chemistry.
Appendix B
(Informative)
Gel permeation chromatography calibration standard solution peak
Figure B.1 gel permeation chromatography calibration standard solution peak
Appendix C
(Informative)
Quantitative ions, auxiliary ions and their ion abundance ratio
Table C.1 Quantitative determination of target, internal standard and substitute ion, auxiliary ion and their ion abundance ratio
Chloride M (M 2) (M 4) (M 6) Ion abundance ratio /
Target
Chlorinated biphenyl 188 190 */3.13 ± 0.47
Dichlorobiphenyl 222 224 * // 1.56 ± 0.23
TCB 256 258 * // 1.04 ± 0.16
Tetrachlorobiphenyl 290 292 */0.77 ± 0.12
Pentachlorobenzene/326 * 328/1.55 ± 0.23
Hexachlorodiphenyl/360 * 362/1.24 ± 0.19
Heptachlorobiphenyl/394 396 */1.05 ± 0.16
OctaBiphenyl/428 430 */0.89 ± 0.13
Nine PCBs/462 464 * 0.77 ± 0.12
Decabromodiphenyl // 498 * 500 1.16 ± 0.17
Alternative PBB-153 308 *, 310, 468
Internal standard
Tetrachloro-xylene
(TCMX)
242, 244 *, 246
*. Quantitative ion
Appendix D
(Informative)
The precision of the method
When the amount of solid waste fly ash sampling was 20.0 g, fly ash solid waste leachate sampling volume of 300 ml, solid waste
The material is extracted by pressurized fluid, the extract is extracted by liquid-liquid extraction, the extract is purified by a multi-layer silica gel column, and the volume of constant volume
Is 1.0 ml, the method of determination of solid waste samples precision (n = 6) in Table D.1, the determination of solid waste leachate sample
The precision of the method (n = 6) is shown in Table D.2.
Table D.1 solid waste sample analysis methods precision summary table
Serial number of the compound name
Total average /
(Μg/kg)
Laboratory relative standard
Quasi-deviation /%
Laboratory relative standard
Quasi-deviation /%
Repeatability limit /
(Μg/kg)
Reproducibility limit /
(Μg/kg)
1 PCB-28
4.41 4.69.2 14 1 2
23.3 5.06.5 4.9 4 5
90.9 5.5 ///
2 PCB-52
4.44 3.89.8 10 1 2
23.0 4.86.5 5.3 4 5
90.8 4.1 ///
3 PCB-101
4.64 4.4  11 12 1 2
23.8 4.65.9 3.2 1 2
89.2 6.4 ///
4 PCB-81
4.86 4.99.2 16 1 3
25.1 3.55.2 7.2 4 6
98.7 8.7 ///
5 PCB-77
4.84 5.012 19 2 3
24.0 3.67.2 5.3 4 5
92.9 5.7 ///
6 PCB-123
4.94 4.69.8 18 1 3
25.6 2.76.0 13 4 10
91.8 4.9 ///
7 PCB-118
4.73 3.8  11 17 1 3
23.2 3.15.6 6.0 3 5
92.0 7.5 ///
8 PCB-114
4.76 4.58.6 15 1 3
23.6 4.06.0 4.7 4 5
88.6 6.7 ///
9 PCB-153
4.78 3.411 13 1 2
23.6 4.86.7 4.4 4 5
103 6.2 ///
10 PCB-105
4.63 3.710 16 1 3
23.2 4.16.3 6.1 4 5
108 8.9 ///
Serial number of the compound name
Total average /
(Μg/kg)
Laboratory relative standard
Quasi-deviation /%
Laboratory relative standard
Quasi-deviation /%
Repeatability limit /
(Μg/kg)
Reproducibility limit /
(Μg/kg)
11 PCB-138
4.38 5.511 14 2 3
24.4 4.26.0 8.0 4 7
95.1 6.9 ///
12 PCB-126
5.02 4.814 19 2 3
24.7 4.25.9 10 4 8
13 PCB-167
4.87 5.110 18 2 3
24.2 4.86.5 9.1 4 7
14 PCB-156
5.15 5.013 22 2 4
25.5 4.56.8 18 5 14
107 6.1 ///
15 PCB-157
4.83 4.810 19 1 3
23.8 4.36.8 8.2 4 7
88.6 4.6 ///
16 PCB-180
4.98 4.213 15 2 3
24.1 3.96.2 9.6 4 8
98.0 7.0 ///
17 PCB-169
5.19 5.315 18 2 3
25.6 3.516 11 8 11
91.9 4.2 ///
18 PCB-189
5.02 4.810 18 1 3
24.8 3.58.2 13 4 10
92.6 3.6 ///
19 PBB-153
20.8 3.812 19 6 12
102 4.29.2 16 18 48
101 4.1 ///
Table D.2 solid waste leachate sample analysis method precision summary table
Serial number of the compound name
Total average /
(Μg/L)
Laboratory relative standard
Quasi-deviation /%
Laboratory relative standard
Quasi-deviation /%
Repeatability limit /
(Μg/L)
Reproducibility limit /
(Μg/L)
1 PCB-28
0.26 4.48.9 16 0.05 0.2
0.98 1019 8.3 0.5 0.5
2 PCB-52
0.25 4.811 12 0.05 0.1
0.98 7.618 6.3 0.5 0.5
3 PCB-101
0.25 5.29.3 16 0.06 0.2
0.93 8.544 11 0.5 0.6
4 PCB-81
0.27 3.811 25 0.06 0.2
1.00 1320 11 0.5 0.5
5 PCB-77
0.27 5.511 29 0.06 0.3
0.99 9.0  19 10 0.4 0.5
6 PCB-123
0.27 5.510 24 0.05 0.2
0.97 8.433 7.9 0.5 0.5
7 PCB-118
0.26 4.113 23 0.06 0.2
0.95 1118 5.9 0.4 0.4
8 PCB-114
0.27 4.1  12 21 0.06 0.2
0.96 9.619 7.0 0.4 0.4
9 PCB-153
0.26 5.39.1 17 0.05 0.2
0.95 9.519 4.6 0.4 0.4
10 PCB-105
0.26 4.1  11 23 0.06 0.2
0.96 1120 6.2 0.4 0.4
11 PCB-138
0.26 4.1  12 21 0.06 0.2
0.96 9.119 6.4 0.4 0.4
12 PCB-126
0.28 4.611 28 0.06 0.3
1.00 8.221 13 0.5 0.6
13 PCB-167
0.29 5.5  18 26 0.06 0.2
0.97 9.220 9.1 0.4 0.5
14 PCB-156
0.27 4.716 29 0.06 0.3
1.00 1021 13 0.5 0.6
15 PCB-157
0.27 3.815 26 0.06 0.2
0.97 1020 9.4 0.4 0.5
16 PCB-180
0.26 4.712 20 0.06 0.2
0.95 1021 6.8 0.4 0.4
17 PCB-169
0.29 5.59.9 24 0.06 0.3
1.01 1222 14 0.5 0.6
18 PCB-189
0.27 4.3  13 22 0.06 0.2
0.96 1121 12 0.5 0.5
19 PBB-153
1.11 4.611 33 0.3 2
3.55 1121 38 2 5
Appendix E
(Informative)
The accuracy of the method
When the amount of solid waste fly ash sampling was 20.0 g, fly ash solid waste leachate sampling volume of 300 ml, solid waste
The material is extracted by pressurized fluid, the extract is extracted by liquid-liquid extraction, the extract is purified by a multi-layer silica gel column, and the volume of constant volume
1.0 ml, the solid waste sample spike recovery and other accuracy indicators in Table E.1, solid waste leachate sample plus
The standard indexes such as standard recovery rate are shown in Table E.2.
Table E.1 solid waste sample analysis accuracy summary table
Serial number of the compound name
Scalar /
(μg/kg)
Spike recovery
range/%
P /% PS /% 2 PP S /%
1 PCB-28
25.0 85.9 ~ 100 93.1 4.6 93.1 ± 9.2
100 84.6 ~ 98.4 ///
2 PCB-52
25.0 83.5 ~ 99.6 92.0 4.9 92.0 ± 9.8
100 84.6 ~ 95.7 ///
3 PCB-101
25.0 90.0 ~ 98.6 94.3 3.0 94.3 ± 6.0
100 80.9 ~ 97.6 ///
4 PCB-81
25.0 91.7 ~ 111 100 7.2 100 ± 14
100 87.9 ~ 111 ///
5 PCB-77
25.0 91.3 ~ 106 95.9 5.1 95.9 ± 10
100 87.6 ~ 102 ///
6 PCB-123
25.0 90.5 ~ 129 103 13.2 103 ± 26
100 87.0 ~ 99.0 ///
7 PCB-118
25.0 84.0 ~ 99.1 92.9 5.5 92.9 ± 11
100 81.6 ~ 99.6 ///
8 PCB-114
25.0 88.4 ~ 99.0 94.5 4.4 94.5 ± 8.8
100 79.0 ~ 95.5 ///
9 PCB-153
25.0 88.1 ~ 98.6 94.3 4.2 94.3 ± 8.4
100 94.8 ~ 112 ///
10 PCB-105
25.0 82.5 ~ 99.5 92.6 5.7 92.6 ± 11
100 96.7 ~ 121 ///
11 PCB-138
25.0 89.3 ~ 110 97.5 7.8 97.5 ± 15
100 88.7 ~ 107 ///
12 PCB-126
25.0 89.3 ~ 114 98.7 10.3 98.7 ± 20
100 91.5 ~ 121 ///
13 PCB-167
25.0 87.7 ~ 110 96.9 8.8 96.9 ± 17
100 89.9 ~ 116 ///
Serial number of the compound name
Scalar /
(μg/kg)
Spike recovery
range/%
P /% PS /% 2 PP S /%
14 PCB-156
25.0 85.3 ~ 137 102 18.7 102 ± 37
100 98.7 ~ 117 ///
15 PCB-157
25.0 88.7 ~ 104 95.1 7.8 95.1 ± 15
100 82.7 ~ 94.8 ///
16 PCB-180
25.0 86.3 ~ 110 96.2 9.3 96.2 ± 18
100 89.9 ~ 108 ///
17 PCB-169
25.0 85.7 ~ 121 102 11.6 102 ± 23
100 86.2 ~ 96.4 ///
18 PCB-189
25.0 86.3 ~ 116 99.2 12.7 99.2 ± 25
100 88.7 ~ 97.4 ///
19 PBB-153
100 85.0 ~ 122 102 16.3 102 ± 32
400 96.0 ~ 108 ///
Table E.2 fly ash solid waste leachate sample analysis method accuracy summary table
Serial number of the compound name
Scalar /
(μg/L)
Spike recovery range
/%
P /% PS /% 2 PP S /%
1 PCB-28 1.33 65.8 ~ 81.1 73.8 6.1 73.8 ± 12
2 PCB-52 1.33 68.3 ~ 80.3 73.5 4.6 73.5 ± 9.2
3 PCB-101 1.33 56.1 ~ 77.9 70.2 7.5 70.2 ± 15
4 PCB-81 1.33 65.4 ~ 85.3 75.5 8.0 75.5 ± 16
5 PCB-77 1.33 63.3 ~ 85.3 74.2 7.5 74.2 ± 15
6 PCB-123 1.33 64.2-82.9 73.3 6.6 73.3 ± 13
7 PCB-118 1.33 64.2 ~ 75.9 71.8 4.2 71.8 ± 8.4
8 PCB-114 1.33 64.6 ~ 77.4 72.5 5.1 72.5 ± 10
9 PCB-153 1.33 67.3 ~ 75.3 71.8 3.3 71.8 ± 6.6
10 PCB-105 1.33 65.4 ~ 77.4 72.0 4.5 72.0 ± 9.0
11 PCB-138 1.33 66.3 ~ 77.8 72.3 4.6 72.3 ± 9.2
12 PCB-126 1.33 63.3 ~ 88.8 74.9 9.4 74.9 ± 19
13 PCB-167 1.33 64.9 ~ 80.9 72.6 6.6 72.6 ± 13
14 PCB-156 1.33 64.0 ~ 88.0 74.9 9.9 74.9 ± 19
15 PCB-157 1.33 64.4 ~ 80.9 72.7 6.9 72.7 ± 14
16 PCB-180 1.33 65.6 ~ 76.6 71.5 4.8 71.5 ± 9.6
17 PCB-169 1.33 62.3 ~ 86.8 75.8 10.5 75.8 ± 21
18 PCB-189 1.33 61.8 ~ 81.6 71.9 8.6 71.9 ± 17
19 PBB-153 5.33 55.8 ~ 88.2 73.2 12.6 73.2 ± 25
Related standard:   HJ 892-2017  HJ 874-2017
   
 
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